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The title compound, [Cu2(CH3O)2(C5H5N)4](ClO4)2, consists of a centrosymmetric dinuclear unit with bridging methoxo groups, and each CuII atom forms a square-planar CuN2O2 unit with pyridine ligands. The Cu...Cu distance is 2.9336 (11) Å and the Cu—O—Cu bond angle is 99.51 (7)°. The perchlorate anions are at semi-coordination distances, the Cu—O(perchlorate) distances being in the range 2.649 (2)–2.741 (2) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804018987/ob6400sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804018987/ob6400Isup2.hkl
Contains datablock I

CCDC reference: 251581

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.033
  • wR factor = 0.095
  • Data-to-parameter ratio = 14.7

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.68 Ratio PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors for Cl1 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 1 C22 H26 Cl2 Cu2 N4 O10
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 7 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: CrystalClear (Rigaku, 2002); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Di-µ-methoxobis[dipyridinecopper(II)] diperchlorate top
Crystal data top
[Cu2(CH3O)2(C5H5N)4](ClO4)2F(000) = 716
Mr = 704.45Dx = 1.688 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 8.528 (4) ÅCell parameters from 4713 reflections
b = 16.850 (9) Åθ = 3.2–27.5°
c = 10.185 (6) ŵ = 1.79 mm1
β = 108.697 (8)°T = 293 K
V = 1386.3 (13) Å3Block, purple
Z = 20.38 × 0.32 × 0.24 mm
Data collection top
Rigaku Mercury CCD
diffractometer
2666 independent reflections
Radiation source: rotating-anode generator2230 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.032
ω scanθmax = 26.0°, θmin = 3.2°
Absorption correction: multi-scan
(CrystalClear; Rigaku, 2002)
h = 910
Tmin = 0.512, Tmax = 0.651k = 2020
8628 measured reflectionsl = 1210
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.033Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.096H-atom parameters constrained
S = 1.09 w = 1/[σ2(Fo2) + (0.0576P)2]
where P = (Fo2 + 2Fc2)/3
2666 reflections(Δ/σ)max = 0.001
181 parametersΔρmax = 0.49 e Å3
0 restraintsΔρmin = 0.31 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cu10.90756 (3)0.562718 (16)0.90737 (3)0.03488 (14)
O10.86813 (19)0.46463 (9)0.98686 (16)0.0331 (4)
N10.9723 (2)0.66512 (12)0.8416 (2)0.0379 (5)
N20.6698 (3)0.58083 (12)0.7970 (2)0.0392 (5)
C11.0324 (3)0.72423 (16)0.9298 (3)0.0492 (7)
H11.04520.71661.02310.059*
C21.0766 (4)0.79631 (17)0.8884 (3)0.0568 (8)
H21.11560.83700.95230.068*
C31.0623 (3)0.80729 (16)0.7514 (3)0.0528 (7)
H31.09340.85500.72120.063*
C41.0013 (3)0.74628 (16)0.6603 (3)0.0497 (7)
H40.98940.75220.56680.060*
C50.9579 (3)0.67644 (15)0.7084 (3)0.0435 (6)
H50.91690.63530.64590.052*
C60.5932 (3)0.64982 (16)0.8013 (3)0.0472 (7)
H60.65300.69010.85800.057*
C70.4306 (3)0.66379 (18)0.7260 (3)0.0552 (8)
H70.38250.71280.73110.066*
C80.3394 (4)0.6045 (2)0.6430 (3)0.0555 (8)
H80.22850.61210.59220.067*
C90.4169 (4)0.5339 (2)0.6375 (3)0.0564 (8)
H90.35890.49320.58080.068*
C100.5797 (3)0.52302 (16)0.7153 (3)0.0473 (6)
H100.62940.47430.71160.057*
C110.7315 (3)0.44901 (16)1.0326 (3)0.0473 (7)
H11A0.73850.39561.06700.071*
H11B0.63080.45530.95670.071*
H11C0.73220.48541.10530.071*
Cl10.99299 (8)0.39356 (4)0.71571 (6)0.04589 (19)
O20.9520 (3)0.47617 (11)0.70503 (19)0.0533 (5)
O31.1126 (2)0.37655 (11)0.84887 (19)0.0520 (5)
O40.8448 (3)0.34862 (14)0.7021 (3)0.0852 (8)
O51.0592 (3)0.37216 (17)0.6100 (2)0.0889 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0319 (2)0.0314 (2)0.0395 (2)0.00015 (11)0.00879 (14)0.00644 (11)
O10.0296 (8)0.0348 (9)0.0350 (9)0.0011 (7)0.0107 (7)0.0055 (7)
N10.0364 (11)0.0349 (11)0.0398 (11)0.0003 (9)0.0088 (9)0.0067 (9)
N20.0352 (11)0.0361 (11)0.0438 (12)0.0043 (9)0.0092 (9)0.0064 (9)
C10.0582 (17)0.0474 (16)0.0388 (14)0.0075 (13)0.0112 (13)0.0021 (12)
C20.065 (2)0.0434 (16)0.0581 (18)0.0148 (14)0.0150 (15)0.0043 (13)
C30.0467 (16)0.0423 (16)0.0697 (19)0.0001 (13)0.0192 (15)0.0209 (14)
C40.0567 (17)0.0482 (16)0.0456 (15)0.0065 (13)0.0185 (13)0.0123 (12)
C50.0473 (15)0.0390 (14)0.0429 (14)0.0042 (12)0.0124 (12)0.0039 (11)
C60.0399 (14)0.0380 (15)0.0652 (18)0.0019 (11)0.0190 (14)0.0020 (12)
C70.0469 (17)0.0481 (16)0.073 (2)0.0171 (14)0.0227 (15)0.0181 (15)
C80.0378 (15)0.080 (2)0.0449 (16)0.0158 (15)0.0077 (13)0.0103 (15)
C90.0427 (16)0.072 (2)0.0490 (17)0.0025 (14)0.0076 (13)0.0138 (15)
C100.0414 (14)0.0441 (16)0.0509 (16)0.0055 (12)0.0071 (12)0.0031 (13)
C110.0358 (14)0.0545 (17)0.0538 (16)0.0046 (12)0.0175 (13)0.0093 (13)
Cl10.0482 (4)0.0463 (4)0.0390 (4)0.0105 (3)0.0082 (3)0.0074 (3)
O20.0673 (13)0.0442 (11)0.0472 (11)0.0167 (10)0.0167 (10)0.0044 (9)
O30.0544 (11)0.0545 (12)0.0409 (10)0.0144 (9)0.0068 (9)0.0002 (8)
O40.0633 (15)0.0685 (16)0.104 (2)0.0160 (12)0.0004 (13)0.0033 (13)
O50.0945 (17)0.127 (2)0.0452 (13)0.0517 (16)0.0227 (12)0.0132 (13)
Geometric parameters (Å, º) top
Cu1—O11.9170 (18)C4—C51.371 (4)
Cu1—O1i1.9263 (18)C4—H40.9300
Cu1—N11.992 (2)C5—H50.9300
Cu1—N22.002 (2)C6—C71.373 (4)
Cu1—O22.649 (2)C6—H60.9300
Cu1—O3i2.741 (2)C7—C81.377 (4)
Cu1—Cu1i2.9336 (11)C7—H70.9300
O1—C111.411 (3)C8—C91.371 (4)
O1—Cu1i1.9263 (18)C8—H80.9300
N1—C11.329 (3)C9—C101.372 (4)
N1—C51.336 (3)C9—H90.9300
N2—C61.341 (3)C10—H100.9300
N2—C101.350 (3)C11—H11A0.9600
C1—C21.377 (4)C11—H11B0.9600
C1—H10.9300C11—H11C0.9600
C2—C31.374 (4)Cl1—O51.413 (2)
C2—H20.9300Cl1—O21.431 (2)
C3—C41.371 (4)Cl1—O31.4404 (19)
C3—H30.9300Cl1—O41.441 (2)
O1—Cu1—O1i80.49 (7)C4—C3—H3120.7
O1—Cu1—N1173.69 (7)C2—C3—H3120.7
O1i—Cu1—N193.60 (8)C3—C4—C5119.3 (3)
O1—Cu1—N294.90 (8)C3—C4—H4120.4
O1i—Cu1—N2174.91 (7)C5—C4—H4120.4
N1—Cu1—N291.08 (9)N1—C5—C4122.6 (3)
O1—Cu1—O286.68 (7)N1—C5—H5118.7
O1i—Cu1—O286.52 (7)C4—C5—H5118.7
N1—Cu1—O295.22 (8)N2—C6—C7123.1 (3)
N2—Cu1—O291.08 (8)N2—C6—H6118.5
O1—Cu1—O3i82.47 (7)C7—C6—H6118.5
O1i—Cu1—O3i85.53 (7)C6—C7—C8119.3 (3)
N1—Cu1—O3i94.92 (8)C6—C7—H7120.4
N2—Cu1—O3i96.05 (8)C8—C7—H7120.4
O2—Cu1—O3i167.47 (6)C9—C8—C7118.1 (3)
O1—Cu1—Cu1i40.36 (5)C9—C8—H8121.0
O1i—Cu1—Cu1i40.13 (5)C7—C8—H8121.0
N1—Cu1—Cu1i133.69 (6)C8—C9—C10120.2 (3)
N2—Cu1—Cu1i135.23 (6)C8—C9—H9119.9
O2—Cu1—Cu1i85.55 (6)C10—C9—H9119.9
O3i—Cu1—Cu1i82.14 (5)N2—C10—C9122.0 (3)
C11—O1—Cu1125.12 (15)N2—C10—H10119.0
C11—O1—Cu1i123.20 (16)C9—C10—H10119.0
Cu1—O1—Cu1i99.51 (7)O1—C11—H11A109.5
C1—N1—C5118.0 (2)O1—C11—H11B109.5
C1—N1—Cu1120.67 (18)H11A—C11—H11B109.5
C5—N1—Cu1121.34 (17)O1—C11—H11C109.5
C6—N2—C10117.3 (2)H11A—C11—H11C109.5
C6—N2—Cu1122.02 (18)H11B—C11—H11C109.5
C10—N2—Cu1120.68 (18)O5—Cl1—O2109.75 (15)
N1—C1—C2122.6 (3)O5—Cl1—O3109.33 (13)
N1—C1—H1118.7O2—Cl1—O3110.32 (11)
C2—C1—H1118.7O5—Cl1—O4110.19 (18)
C3—C2—C1119.1 (3)O2—Cl1—O4108.57 (14)
C3—C2—H2120.5O3—Cl1—O4108.67 (15)
C1—C2—H2120.5Cl1—O2—Cu1124.67 (10)
C4—C3—C2118.5 (2)
Symmetry code: (i) x2, y+1, z2.
 

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